CN111621033A - Method for extracting humic acid from lavender distillation waste residue - Google Patents
Method for extracting humic acid from lavender distillation waste residue Download PDFInfo
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- CN111621033A CN111621033A CN202010444286.8A CN202010444286A CN111621033A CN 111621033 A CN111621033 A CN 111621033A CN 202010444286 A CN202010444286 A CN 202010444286A CN 111621033 A CN111621033 A CN 111621033A
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- lavender
- waste residue
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- humic acid
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- 239000002699 waste material Substances 0.000 title claims abstract description 44
- 244000178870 Lavandula angustifolia Species 0.000 title claims abstract description 43
- 235000010663 Lavandula angustifolia Nutrition 0.000 title claims abstract description 43
- 239000001102 lavandula vera Substances 0.000 title claims abstract description 43
- 235000018219 lavender Nutrition 0.000 title claims abstract description 43
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000004021 humic acid Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004821 distillation Methods 0.000 title abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 30
- 238000001914 filtration Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- 241000196324 Embryophyta Species 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000010979 pH adjustment Methods 0.000 claims 1
- 238000011085 pressure filtration Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000000605 extraction Methods 0.000 abstract description 6
- 239000000341 volatile oil Substances 0.000 description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000186361 Actinobacteria <class> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241001579180 Matthiola longipetala Species 0.000 description 1
- 235000006679 Mentha X verticillata Nutrition 0.000 description 1
- 235000002899 Mentha suaveolens Nutrition 0.000 description 1
- 235000001636 Mentha x rotundifolia Nutrition 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000001914 calming effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
- C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Soil Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Compounds Of Unknown Constitution (AREA)
Abstract
The invention discloses a method for extracting humic acid from lavender distilled waste residue, which comprises the following steps: step 1: drying and crushing the lavender distilled waste residue, and then carrying out filtering treatment; step 2: mixing the lavender distilled waste residue obtained in the step 1 with a potassium hydroxide solution, and placing the mixture into a high-pressure reaction kettle for reaction; and step 3: filtering the solution obtained after the reaction in the step 2, and collecting filtrate; and 4, step 4: adjusting the pH value of the solution obtained in the step 3 to 6.5-7.0, and standing and settling the solution; and 5: carrying out mechanical treatment on the mixed solution settled in the step (4) to separate solid from liquid, washing and filtering the separated solid, and then drying; the method has the advantages of realizing the extraction of humic acid molecules from the lavender distillation waste residue, along with simple process and low cost.
Description
Technical Field
The invention belongs to solid waste resource utilization, and particularly relates to a method for extracting humic acid from lavender distilled waste residue.
Background
Enterprises in Xinjiang Ili, the largest perfume production base in Asian regions extract lavender essential oil by a steam extraction method, the yield of the lavender essential oil is over 200 tons under the support of a planting area of approximately 5 ten thousand mu of Ili, lavender with fresh and cool aroma and strong and pleasant fragrance is a valuable and important natural perfume plant, and the extracted essential oil has the functions of calming, hypnotizing, spasmolysis, antibiosis and the like. Generally speaking, the volatile essential oil accounts for 1% -3% of the total weight of the herbs, and the waste residue generated by extracting the lavender essential oil by Yili in Xinjiang can reach 2 million tons. In addition, Yili also produces essential oils of citrus, mint, grape seeds, etc., producing a large amount of waste residues.
However, because the Ili climate is dry, the water loss is fast, and the survival of microorganisms such as bacteria, yeasts, fungi, actinomycetes and the like is not facilitated, so that a large amount of water is consumed in the treatment path of the lavender waste residue used as the fertilizer, the cost is high, and the economic benefit is low. The economic benefit of waste residue treatment is not enough and is a common disease for essential oil manufacturers. The waste residue after the extraction of the essential oil is useless and can not be used by people. Farmers living in Yili lavender base need to spend money to hire people to process waste residues, which brings difficulty to production and life.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for extracting humic acid from lavender distilled waste residue, aiming at the problem that the unused and useless lavender distilled waste residue is a potential safety hazard in the environment. According to the method, the lavender distilled waste residue is taken as a starting point, the process of alkali dissolution-acid precipitation is adopted, high-quality humic acid is obtained from the lavender distilled waste residue, the lavender distilled waste residue is expected to be economically, effectively, environmentally and environmentally treated, the used equipment is simple, the operability is high, and a new economic and applicable idea is provided for waste residue treatment of essential oil manufacturers.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for extracting humic acid from lavender distilled waste residue comprises the following steps:
step 1: drying and crushing the lavender distilled waste residue, and then carrying out filtering treatment;
step 2: mixing the lavender distilled waste residue obtained in the step 1 with a potassium hydroxide solution according to the weight ratio of 1-4: mixing the components in a mass ratio of 60, and placing the mixture into a high-pressure reaction kettle for reaction;
and step 3: filtering the solution obtained after the reaction in the step 2, and collecting filtrate;
and 4, step 4: adjusting the pH value of the solution obtained in the step 3 to 6.5-7.0, and standing and settling the solution;
and 5: and 4, mechanically treating the mixed solution settled in the step 4 to separate solid from liquid, washing and filtering the separated solid, and drying.
Preferably, the drying treatment is drying in the shade.
Preferably, the diameter of the sieve in the sieving treatment in the step 1 is 100 meshes.
Preferably, the concentration of the sodium hydroxide solution is 0.5-3 mol/L.
Preferably, the conditions of the high-pressure reaction kettle in the step 2 are 150-200 ℃ and the time is 2-15 h.
Preferably, the filtration in step 3 is performed by using filter paper, and the filter paper is neutral filter paper.
Preferably, phosphoric acid is used for adjusting the pH value in the step 4.
Preferably, the concentration of the phosphoric acid is 0.1 to 2 mol/L.
Preferably, the mechanical treatment comprises one of filter pressing, suction filtration and centrifugation.
Preferably, the plant humic acid is prepared by any one of the processes.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the extraction of humic acid with economic value by utilizing the lavender distillation waste residue is realized;
(2) the method has the advantages of simple equipment and high operability, and provides an economical and applicable new idea for treating the waste residue of an essential oil factory;
drawings
FIG. 1 is a schematic diagram of the extraction process of the present invention;
FIG. 2 is an infrared image of the humic acid product extracted according to the invention;
FIG. 3 is a diagram showing a sample solution obtained by filtration after the reaction in the autoclave.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that the same is not to be considered as limiting the invention
A method for extracting humic acid from lavender distilled waste residue comprises the following steps:
step 1: drying and crushing the lavender distilled waste residue, and then carrying out filtering treatment;
step 2: mixing the lavender distilled waste residue obtained in the step 1 with a potassium hydroxide solution according to the weight ratio of 1-4: mixing the components in a mass ratio of 60, and placing the mixture into a high-pressure reaction kettle for reaction;
and step 3: filtering the solution obtained after the reaction in the step 2, and collecting filtrate;
and 4, step 4: adjusting the pH value of the solution obtained in the step 3 to 6.5-7.0, and standing and settling the solution;
and 5: and 4, mechanically treating the mixed solution settled in the step 4 to separate solid from liquid, washing and filtering the separated solid, and drying.
Preferably, the drying treatment is drying in the shade.
Preferably, the diameter of the sieve in the sieving treatment in the step 1 is 100 meshes.
Preferably, the concentration of the sodium hydroxide solution is 0.5-3 mol/L.
Preferably, the conditions of the high-pressure reaction kettle in the step 2 are 150-200 ℃ and the time is 2-15 h.
Preferably, the filtration in step 3 is performed by using filter paper, and the filter paper is neutral filter paper.
Preferably, phosphoric acid is used for adjusting the pH value in the step 4.
Preferably, the concentration of the phosphoric acid is 0.1 to 2 mol/L.
Preferably, the mechanical treatment comprises one of filter pressing, suction filtration and centrifugation.
Preferably, the plant humic acid prepared by any one of the processes
Example 1
As shown in figure 1, the lavender distilled waste residue is dried in the shade, smashed, processed by a 100-mesh filter sieve, and added into a high-pressure reaction kettle for reaction for 10 hours at 160 ℃ after 60mL of potassium hydroxide solution and 1g of lavender distilled waste residue are uniformly mixed; filtering by filter paper to obtain a grey brown potassium humate solution, adding 1mol/L phosphoric acid solution into the solution to adjust the pH value to 6.5, carrying out mechanical treatment on a reaction product to separate solid from liquid, washing and filtering the solid, and naturally drying in the shade to obtain the humic acid.
Example 2
Smashing the lavender distilled waste residue after drying in the shade, processing by a 100-mesh filter screen, uniformly mixing 60mL of sodium hydroxide solution and 2g of lavender distilled waste residue, adding into a high-pressure reaction kettle, reacting at 160 ℃ for 10 hours, and extracting humic acid in the lavender distilled waste residue; filtering by using filter paper to obtain a grey brown potassium humate solution, adding 1mol/L phosphoric acid solution into the solution to adjust the pH value to 6.5, carrying out mechanical treatment on a reaction product to separate solid from liquid, washing and filtering the solid, and naturally drying in the shade to obtain humic acid extracted from the lavender distillation waste residue.
Example 3
Smashing the lavender distilled waste residue after drying in the shade, processing by a 100-mesh filter screen, uniformly mixing 60mL of sodium hydroxide solution and 3g of lavender distilled waste residue, adding into a high-pressure reaction kettle, reacting at 160 ℃ for 10 hours, and extracting humic acid in the lavender distilled waste residue; filtering by using filter paper to obtain a grey brown potassium humate solution, adding 1mol/L phosphoric acid solution into the solution to adjust the pH value to 6.5, carrying out mechanical treatment on a reaction product to separate solid from liquid, washing and filtering the solid, and naturally drying in the shade to obtain humic acid extracted from the lavender distillation waste residue.
Example 4
Smashing the lavender distilled waste residue after drying in the shade, processing by a 100-mesh filter screen, uniformly mixing 60mL of sodium hydroxide solution and 4g of lavender distilled waste residue, adding into a high-pressure reaction kettle, reacting at 160 ℃ for 10 hours, and extracting humic acid in the lavender distilled waste residue; filtering by using filter paper to obtain a grey brown potassium humate solution, adding 1mol/L phosphoric acid solution into the solution to adjust the pH value to 6.5, carrying out mechanical treatment on a reaction product to separate solid from liquid, washing and filtering the solid, and naturally drying in the shade to obtain humic acid extracted from the lavender distillation waste residue.
The yields of humic acid obtained in examples 1-4 are shown in Table 1, and therefore, the present process was carried out using lavender distilled residue and potassium hydroxide solution 3: the yield of humic acid is highest with a mass ratio of 60; the infrared pattern of the obtained humic acid product is shown in FIG. 2, wherein 3100-3600cm-1 shows a stretching vibration absorption peak of-OH, -NH-, 1790-1680cm-1 shows a vibration absorption peak of-COOH, -C-O-, 1250cm-1 shows a stretching vibration absorption peak of phenolic hydroxyl group and alcoholic hydroxyl aliphatic bond, and the product is proved to be humic acid.
TABLE 1 extraction yield of humic acid
Claims (10)
1. The method for extracting humic acid from lavender distilled waste residue is characterized by comprising the following steps:
step 1: drying and crushing the lavender distilled waste residue, and then carrying out filtering treatment;
step 2: mixing the lavender distilled waste residue obtained in the step 1 with a potassium hydroxide solution according to the weight ratio of 1-4: mixing the components in a mass ratio of 60, and placing the mixture into a high-pressure reaction kettle for reaction;
and step 3: filtering the solution obtained after the reaction in the step 2, and collecting filtrate;
and 4, step 4: adjusting the pH value of the solution obtained in the step 3 to 6.5-7.0, and standing and settling the solution;
and 5: and 4, mechanically treating the mixed solution settled in the step 4 to separate solid from liquid, washing and filtering the separated solid, and drying.
2. The method of claim 1, wherein the drying process is drying in the shade.
3. The method as claimed in claim 1, wherein the sieve of step 1 has a diameter of 100 mesh.
4. The method according to claim 1, wherein the concentration of the sodium hydroxide solution is 0.5 to 3 mol/L.
5. The method as claimed in claim 1, wherein the high pressure reaction kettle in step 2 is at a temperature of 150 ℃ and 200 ℃ for 2-15 h.
6. The method according to claim 1, wherein the filtering in step 3 is performed by using filter paper, and the filter paper is neutral filter paper.
7. The method of claim 1, wherein the pH adjustment in step 4 is performed using phosphoric acid.
8. The method of claim 7, wherein the phosphoric acid concentration is 0.1 to 2 mol/L.
9. The method of claim 1, wherein the mechanical treatment comprises one of pressure filtration, suction filtration, and centrifugation.
10. Plant humic acid produced by the process of any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010444286.8A CN111621033A (en) | 2020-05-22 | 2020-05-22 | Method for extracting humic acid from lavender distillation waste residue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010444286.8A CN111621033A (en) | 2020-05-22 | 2020-05-22 | Method for extracting humic acid from lavender distillation waste residue |
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| CN111621033A true CN111621033A (en) | 2020-09-04 |
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| CN202010444286.8A Pending CN111621033A (en) | 2020-05-22 | 2020-05-22 | Method for extracting humic acid from lavender distillation waste residue |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949249A (en) * | 2016-06-27 | 2016-09-21 | 赣州华汉生物科技有限公司 | Method for extracting lavandula angustifolia flavone from lavandula angustifolia pulp water |
| CN106047500A (en) * | 2016-05-31 | 2016-10-26 | 铜仁职业技术学院 | Method for efficiently extracting lavender and application of extract of lavender |
| CN106478961A (en) * | 2016-10-12 | 2017-03-08 | 西安兰心有机肥有限公司 | Plant humic acid and its manufacture craft |
-
2020
- 2020-05-22 CN CN202010444286.8A patent/CN111621033A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106047500A (en) * | 2016-05-31 | 2016-10-26 | 铜仁职业技术学院 | Method for efficiently extracting lavender and application of extract of lavender |
| CN105949249A (en) * | 2016-06-27 | 2016-09-21 | 赣州华汉生物科技有限公司 | Method for extracting lavandula angustifolia flavone from lavandula angustifolia pulp water |
| CN106478961A (en) * | 2016-10-12 | 2017-03-08 | 西安兰心有机肥有限公司 | Plant humic acid and its manufacture craft |
Non-Patent Citations (2)
| Title |
|---|
| 古丽妮尕尔·阿布力克木等: ""薰衣草残渣化学成分及其生物活性"", 《中成药》 * |
| 梁浩等: ""铜仁地区薰衣草残渣化学成分的GC-MS分析"", 《化工管理》 * |
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